CN110988093A - Method for detecting content of high-salt blood cardiovascular drug - Google Patents
Method for detecting content of high-salt blood cardiovascular drug Download PDFInfo
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- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
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- G—PHYSICS
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- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
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Abstract
The invention aims to provide a method for detecting the content of cardiovascular drugs in high-salt blood, so as to overcome the problems in the detection of nitrendipine, nimodipine and nifedipine by using a high-salt blood sample at present. The method of the invention realizes high-sensitivity and high-selectivity detection of any high-salt sample with electrochemical signals. The method is further applied to the quality control of the pharmaceutical preparation and the research of the drug metabolism, has the advantages of simplicity, rapidness, stability, low cost, high enrichment efficiency and the like compared with the traditional chromatographic enrichment separation, is expected to be applied to the quality control of the pharmaceutical preparation and becomes an auxiliary means for the research of complex biological samples.
Description
Technical Field
The invention belongs to the technical field of detection of medicine components and contents, and particularly relates to a method for detecting the content of a cardiovascular medicine in high-salt blood.
Background
The epidemic trend of cardiovascular diseases in China is obvious, so that the morbidity and the mortality of the cardiovascular diseases are increased year by year. Nitrendipine (NT), Nimodipine (NM), and Nifedipine (NF). The blood contains salt, the electrical conductivity is high, and if the sample is not pretreated, the sample is difficult to separate by using the traditional field amplification sample injection method. The pH modulation stacking method overcomes the defects of the traditional field amplification sample feeding method, and avoids the de-stacking phenomenon caused by the fact that the electric conductance of a sample zone is higher than that of a buffer solution. The current chromatographic methods for measuring cardiovascular drugs comprise a liquid chromatography-mass spectrometry combined method, a liquid chromatography and a micelle electrokinetic chromatography. The liquid chromatography and the mass spectrometry have higher requirements on the detector, and the common micelle electrokinetic chromatography cannot meet the detection and separation of complex biological samples due to small enrichment factors and low detection sensitivity.
Disclosure of Invention
The invention aims to provide a method for detecting the content of a high-salt blood central vessel drug, so as to overcome the problems in the detection of Nitrendipine (NT), Nimodipine (NM) and Nifedipine (NF) by a high-salt blood sample at present.
The detection method comprises the following steps:
1) pretreatment of samples
Firstly, standing and centrifuging a blood sample to be detected, which is added with an anticoagulant, at 30 ℃, then centrifuging for 10min at 3000r/min, and taking supernatant; adding methanol (the adding amount of the methanol is 50% of the volume of the supernatant), performing vortex mixing, performing ultrasonic treatment, centrifuging ultrasonic liquid (centrifuging at 3000r/min for 10min), taking supernatant, and blowing the residual methanol by nitrogen to obtain a sample to be detected;
2) dual enrichment Process
Filling a capillary of a capillary electrophoresis apparatus with a separation buffer solution, wherein the preparation method of the separation buffer solution comprises the following steps: firstly, 30mmol/L of Na2B4O7Solution and 1mmol/L Na2HPO4The solution was adjusted to pH 9.10 in sample buffer, and then the sample buffer, SDS and methanol were adjusted to 2Preparing MEKC separation buffer solution according to the volume ratio of 2:7: 1;
introducing the sample to be detected prepared in the step 1) into a capillary tube by electromigration, wherein the electrophoresis power supply uses positive high voltage, the sample introduction voltage is 15kV, and the sample introduction time is 60 s; then, adding a phosphoric acid solution with the pH value of 3.12 in an electric sample injection mode, and injecting the phosphoric acid solution for 80 s; then putting the capillary positive electrode into a separation buffer solution, and separating under positive high pressure of 20 kV;
3) quantitative detection
Carrying out regression analysis on the peak current and the concentration of each analyte according to the regression equation of the nitrendipine, the nimodipine and the nifedipine standard substance to obtain the content of the nitrendipine, the nimodipine and the nifedipine in the blood sample to be detected;
wherein the regression equation of nitrendipine is as follows: y (mg/L) ═ 0.71x (ma) + 0.041;
the regression equation for nimodipine is as follows: y (mg/L) ═ 0.58x (ma) + 0.033;
the regression equation for nifedipine is as follows: y (mg/L) ═ 0.67x (ma) + 0.038.
The method of the invention realizes high-sensitivity and high-selectivity detection of any high-salt sample with electrochemical signals. The method is further applied to the quality control of the pharmaceutical preparation and the research of the drug metabolism, has the advantages of simplicity, rapidness, stability, low cost, high enrichment efficiency and the like compared with the traditional chromatographic enrichment separation, is expected to be applied to the quality control of the pharmaceutical preparation and becomes an auxiliary means for the research of complex biological samples.
Drawings
FIG. 1: a self-assembled capillary electrophoresis system diagram;
FIG. 2: a field amplification sample introduction method separation chart;
FIG. 3: the method enriches and separates an electrophoresis spectrogram.
Detailed Description
The present invention will be described in detail with reference to examples.
Example 1: establishment of a detection System
The needle of the disposable syringe was cut off about 4cm of metal needle, leaving about 1cm of metal tubing. The sample port of the capillary was passed through the metal tube end of the needle and the sample port was placed about 5cm from the metal tube. The capillary tube was then securely sealed with paraffin wax at the location of the metal orifice to facilitate cleaning of the capillary tube with a syringe. The sample inlet port of the capillary tube and the anode of the high-voltage power supply are inserted into a beaker filled with electrophoresis buffer solution, and the outlet end of the capillary tube is fixed on the detection cell by paraffin. The negative electrode of the high-voltage power supply is communicated with the detection pool. The capillary filled with running buffer and the high voltage power supply form a loop to form a separation system, as shown in FIG. 1. Before each operation, the capillary is washed for 3min by 0.1mol/L hydrochloric acid solution, redistilled water and 0.1mol/L sodium hydroxide solution and redistilled water in turn, and then the capillary is separated by MEKC under the separation voltage until the current in the capillary is stable, so that the obtained electroosmotic flow (EOF) is relatively stable, and the reproducibility of the invention is improved.
In the method, Nitrendipine (NT), Nimodipine (NM) and Nifedipine (NF) rapidly migrate and accumulate at the interface of a sample zone and a separation buffer solution under high field strength to achieve first enrichment. Meanwhile, SDS in the micelle enters the sample zone to scan sample ions, so that the length of the sample zone is greatly shortened, and the second enrichment of the sample is realized. Not only realizes the pH modulation stacking combined scavenging micelle electrokinetic chromatography composite enrichment.
The method comprises the following steps:
1) pretreatment of samples
Firstly, standing and centrifuging a blood sample to be detected, which is added with an anticoagulant, at 30 ℃, then centrifuging for 10min at 3000r/min, and taking supernatant; adding methanol (the adding amount of the methanol is 50% of the volume of the supernatant), performing vortex mixing, performing ultrasonic treatment, centrifuging ultrasonic liquid (centrifuging at 3000r/min for 10min), taking supernatant, and blowing the residual methanol by nitrogen to obtain a sample to be detected;
2) dual enrichment Process
Filling a capillary of a capillary electrophoresis apparatus with a separation buffer solution, wherein the preparation method of the separation buffer solution comprises the following steps: firstly, 30mmol/L of Na2B4O7Solution and 1mmol/L Na2HPO4Blending of solutionAdding a sample buffer solution with the pH value of 9.10, and preparing a MEKC separation buffer solution from the sample buffer solution in a volume ratio of 22:7:1 (the sample buffer solution: 23mmol/L SDS: methanol);
introducing the sample to be detected prepared in the step 1) into a capillary tube by electromigration, wherein the electrophoresis power supply uses positive high voltage, and the sample introduction time is 60 s; then, adding a phosphoric acid solution with the pH value of 3.12 in an electric sample injection mode, and injecting the phosphoric acid solution for 80 s; then putting the capillary positive electrode into a separation buffer solution, and separating under positive high pressure of 20 kV;
3) quantitative detection
Carrying out regression analysis on the peak current and the concentration of each analyte according to the regression equation of the nitrendipine, the nimodipine and the nifedipine standard substance to obtain the content of the nitrendipine, the nimodipine and the nifedipine in the blood sample to be detected;
wherein the regression equation of nitrendipine is as follows: y (mg/L) ═ 0.71x (ma) + 0.041;
the regression equation for nimodipine is as follows: y (mg/L) ═ 0.58x (ma) + 0.033;
the regression equation for nifedipine is as follows: y (mg/L) ═ 0.67x (ma) + 0.038.
The optimization steps of the steps are as follows:
1. optimization of sample injection voltage
The influence of the sample injection voltage on the migration time of each analyte is inspected in the range of 9-18 kV, the migration time of the sample is closely related to the voltage, but the voltage is increased, and the detection limit is also increased due to the substrate noise. The low injection voltage can improve the resolution of the measured object, but the low injection voltage can increase the migration time and widen the peak shape. The peak shape is best when the sample injection voltage is 15kV, and the separation degree is maximum. When the sample introduction voltage is increased again, the peak height of the sample is increased but the baseline separation cannot be achieved, so that 15kV is selected as the sample introduction voltage.
2. Selection of concentration and acidity of neutralizer and conductivity reducer
The invention analyzes H3BO3And H3PO4Influence of the pH value of the system and the concentration of each component on the enrichment effect. After the sample injection is finished, the sample is added with 100mmol/L H3BO3(pH 5.1)) And the sample enrichment efficiency is not high. It can be seen that the pH of the acid is less than 5.1 and does not act to neutralize OH "and reduce conductivity. Thus selecting H3PO4According to the system, the enrichment effect of phosphoric acid when the pH value is continuously reduced within the range of 5.0-2.0 is inspected, the enrichment effect is the highest when the concentration of the phosphoric acid is 100mmol/L (pH value is 3.12), the concentration of H & lt + & gt is increased along with the reduction of the pH value, cations on the wall of a capillary tube are replaced, and the phenomenon of peak broadening is gradually obvious. Therefore, the invention adopts 100mmol/L phosphoric acid solution (pH value is 3.12) as the neutralizing agent and the conductivity reducing agent to improve the enrichment efficiency of the sample.
3. Surfactant scavenging mechanism
According to the invention, an anionic surfactant SDS is used for capturing an oncoming weak base sample, and the sample and the micelle move towards the anode together, so that the zone length of the sample is greatly reduced, and the sample is subjected to secondary enrichment.
The peak of three substances can be detected by adding a certain amount of SDS anionic surfactant into a 30mmol/L Na2B4O7-1 mmol/L Na2HPO 4-3.3% methanol background buffer solution with the pH value of 9.10. The separation and enrichment of analytes with different concentrations of SDS (9, 16, 23, 30 and 37mmol/L) was examined. At a SDS concentration of 37mmol/L, the three species had not achieved baseline separation, so an optimal concentration of SDS of 23mmol/L was chosen.
4. Electroosmotic flow regulator
In the buffer solution of pH 9.10, the dissociation degree of silicon hydroxyl groups at the capillary wall increases, the electroosmotic flow also increases, the overall moving speed of the electroosmotic flow driving liquid increases, and the sample reaches the detection end when the complete separation is not achieved. Therefore, organic solvents are required to be added to adjust the electroosmotic flow rate, and different organic solvents have different dielectric constants and generate different electroosmotic flows. The influence of three different regulators such as methanol, isopropanol and ethanol with different concentrations on the separation degree is examined. The results show that the three substances can cause the great reduction of electroosmotic flow, the peak time is prolonged, and the methanol greatly improves the separation degree of the analytes. This is because methanol not only reduces electroosmotic flow by changing the pKa of the silicon hydroxyl groups, but also acts to improve analyte resolution by adjusting the partition coefficient of the analyte in the micelles and mobile phase. The peak appearance was examined when the methanol volume fraction was 1.3%, 2.3%, 3.3% and 4.3%, respectively, and the methanol volume fraction was selected to be 3.3% in consideration of the separation efficiency and the analysis time.
The sample injection time of the phosphoric acid solution is examined within the range of 20-100 s under the condition that the sample injection time of the fixed sample is 60s, and the best sensitivity is achieved when the acid is injected for 80 s. Nitrendipine (NT), Nimodipine (NM) and Nifedipine (NF) rapidly migrate and accumulate at the interface of a sample zone and a separation buffer solution under high field strength to achieve first enrichment. Meanwhile, SDS in the micelle enters the sample zone to scan sample ions, so that the length of the sample zone is greatly shortened, and the second enrichment of the sample is realized. Not only realizes the pH modulation stacking combined scavenging micelle electrokinetic chromatography composite enrichment. The linear regression equation and the correlation coefficient are shown in table 1.
Wherein the regression equation of nitrendipine is as follows: y (mg/L) ═ 0.71x (ma) + 0.041;
the regression equation for nimodipine is as follows: y (mg/L) ═ 0.58x (ma) + 0.033;
the regression equation for nifedipine is as follows: y (mg/L) ═ 0.67x (ma) + 0.038.
The capillary tube length limits the sensitivity of kinetic injection, and the volume of pH modulated stacking-sweeping sample injection is generally 20% or 22% of the tube length. The influence of sample injection time is inspected in the range of 40-90 s (15kV), and the phenomenon that the peak is widened due to overlong sample injection time is found, so that the sample injection time is selected to be 60 s. After the sample introduction is finished, the phosphoric acid solution with the pH value of 3.12 is electrically introduced, H + enters the sample zone, so that the conductivity of the sample zone is reduced, and the sample is electrochemically accumulated. When the sample injection voltage is 15kV, the ratio of the sample injection time to the electrokinetic sample injection time of the acid is studied. The sample injection time of the acid is examined within the range of 20-100 s under the condition that the sample injection time is fixed to be 60s, and the best sensitivity is achieved when the acid is injected for 80 s. The capillary positive electrode was then placed in the separation buffer and separated under a positive high pressure of 20 kV.
Table 1: linear relationship and detection limit table of NM, NF and NT
Under optimized conditions, the reproducibility of the pH modulated stacking-MEKC enrichment method is evaluated by a method of continuously feeding standard mixed solutions of NT, NM and NF (each analyte concentration is 2.0mg/L) for 6 times. RSD of peak height and migration time of each component are respectively 2.1 percent and 0.5 percent (NM); 2.6%, 0.7% (NF) and 2.3%, 0.9% (NT). The inventive result further verifies the feasibility of the method.
In order to verify the practicability of the continuous pre-enrichment technology, the invention compares an electrophoresis spectrogram separated by a traditional field amplification method (see figure 3) with an electrophoresis spectrogram separated by the method (see figure 2), and finds that the peak height and the separation efficiency of the latter are superior to those of the former. The sample enrichment occurs in pH modulation stacking sample injection and micelle sweeping electrophoresis, and the detection sensitivity of the method is (1.8-2.1) multiplied by 10 separated by the traditional field amplification method2And (4) doubling.
Example 2: detection of blood samples
Taking blood from elbow vein of healthy subject on empty stomach, placing blank blood sample and blood sample added with three kinds of drug standard solutions into two centrifuge tubes respectively, adding heparin sodium anticoagulant, standing at 30 ℃, centrifuging at 3000r/min for 10min, taking supernatant into another centrifuge tube, adding methanol solution accounting for 50% of supernatant volume, vortex mixing, performing ultrasonic treatment, centrifuging at 3000r/min for 10min, taking supernatant, blowing nitrogen at 37 ℃ for drying residual methanol, and refrigerating in refrigerator at-20 ℃ for later use.
The capillary is filled with separation buffer solution, then the sample is introduced into the capillary by electromigration, the electrophoresis power supply uses positive high voltage, and then a section of phosphoric acid solution with pH value of 3.12 is introduced by adopting an electric sample introduction mode. The hydrogen ions in the strong acid neutralize the hydroxyl ions in the sample solution, the conductivity of the sample zone is reduced, the component to be detected rapidly migrates and accumulates at the interface of the sample zone and the separation buffer solution under high field intensity to achieve enrichment, and simultaneously SDS in the micelle enters the sample zone to sweep the sample ions, so that the length of the sample zone is shortened
Greatly shortened and secondary enrichment of the sample is realized. The sample solution is injected for 60s and the analyte rapidly migrates into the capillary where it accumulates at the interface of the sample zone and the buffer solution. As the sample is introduced, a phosphoric acid solution of pH3.12 is injected for 80 seconds. The whole sample injection process uses positive high voltage of 15kV, and then the capillary positive electrode is put into separation buffer solution to be separated under positive high voltage of 20 kV. The method is applied to the determination of three drugs in the blood of healthy people, the three drugs are not detected in the result, 2mg/L standard substance solutions of the three drugs are respectively added into the blood of healthy people, and the processing mode is shown in 1.2. The other components of the blood sample do not interfere with the detection of the three analytes. The content of NM, NF and NT in blood and the recovery rate of the added standard are shown in Table 2, the recovery rate is between 95.8 and 103.5 percent, and the relative standard deviation is between 1.2 and 3.9 percent. The test results show that the method has good accuracy, sensitivity and reproducibility, and provides a good quantitative method for analyzing the blood concentration of the human body.
TABLE 2 NM, NF and NT blood levels and normalized recovery (n ═ 5)
Example 3: testing of pharmaceutical tablets
The method is used for measuring three drug tablet samples, the content of the three drugs in the drug tablet samples is respectively 9.86 mg/tablet, 9.92 mg/tablet and 9.79 mg/tablet, the content is basically consistent with the content (10 mg/tablet) marked by a manufacturer, and the relative standard deviation is between 2.1 and 3.2 percent.
Using pH modulation stacking method, after sample is electrically injected, a section of phosphoric acid solution with pH value of 3.12 is electrically injected, and H in the phosphoric acid solution is injected+Neutralize OH in the sample solution-Creating a zone of neutral sample, such that the conductance of the zone is substantially reduced and the sample is separated from the zoneThe migration rate of the molecules is accelerated and the molecules accumulate at the interface between the sample zone and the micellar buffer. SDS with negative charges in the micelle enters a sample area to sweep sample ions, so that the length of the sample area is greatly shortened, and secondary enrichment of the sample is realized. In the invention, positive high voltage is always used, and the direction of the electrode is always unchanged, so that the operation process is simpler.
Claims (5)
1. A method for detecting the content of cardiovascular drugs in high-salt blood is characterized by comprising the following steps:
1) pretreatment of samples
Firstly, standing and centrifuging a blood sample to be detected, which is added with an anticoagulant, and taking a supernatant; adding methanol (ultrasonic after vortex mixing, centrifuging ultrasonic liquid, taking supernatant, blowing the residual methanol by nitrogen, and taking the residual methanol as a sample to be detected;
2) dual enrichment Process
Filling a capillary of a capillary electrophoresis apparatus with a separation buffer solution, wherein the preparation method of the separation buffer solution comprises the following steps: firstly, 30mmol/L of Na2B4O7Solution and 1mmol/L Na2HPO4Adjusting the solution to be a sample buffer solution with the pH value of 9.10, and preparing a MEKC separation buffer solution from the sample buffer solution, SDS and methanol in a volume ratio of 22:7: 1;
then, introducing the sample to be detected prepared in the step 1) into a capillary tube in an electromigration mode; then, adding a phosphoric acid solution with the pH value of 3.12 in an electric sample injection mode, and injecting the phosphoric acid solution for 80 s; then putting the capillary positive electrode into a separation buffer solution, and separating under positive high pressure of 20 kV;
3) quantitative detection
Carrying out regression analysis on the peak current and the concentration of each analyte according to the regression equation of the nitrendipine, the nimodipine and the nifedipine standard substance to obtain the content of the nitrendipine, the nimodipine and the nifedipine in the blood sample to be detected;
wherein the regression equation of nitrendipine is as follows: y (mg/L) ═ 0.71x (ma) + 0.041;
the regression equation for nimodipine is as follows: y (mg/L) ═ 0.58x (ma) + 0.033;
the regression equation for nifedipine is as follows: y (mg/L) ═ 0.67x (ma) + 0.038.
2. The method according to claim 1, wherein the blood sample to be tested in step 1) is left to stand at 30 ℃ after being left to stand for centrifugation, and then centrifuged at 3000r/min for 10 min.
3. The method of claim 1, wherein methanol is added in step 1) in an amount of 50% by volume of the supernatant.
4. The method of claim 1, wherein the ultrasound liquid in step 1) is centrifuged under conditions of 3000r/min for 10 min.
5. The method as claimed in claim 1, wherein the sample to be tested is introduced into the capillary tube in step 2) by electromigration, the electrophoresis power supply is at high positive voltage, the sample introduction voltage is 15kV, and the sample introduction time is 60 s.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1916602A (en) * | 2005-08-19 | 2007-02-21 | 上海市公安局刑事侦查总队 | Capillary electrophoresis method for detecting medications and poisons in blood and urine at the same time |
| US20080020386A1 (en) * | 2006-03-29 | 2008-01-24 | Medigen Biotechnology Corporation | Methods and apparatus for genotyping |
| CN108535349A (en) * | 2018-04-09 | 2018-09-14 | 天津农学院 | A kind of method of NO3-N and NO2-N in quick detection fruits and vegetables and meat products |
| CN109709198A (en) * | 2018-12-29 | 2019-05-03 | 杭州师范大学 | A kind of on-line preconcentration method of Capillary Electrophoresis |
-
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1916602A (en) * | 2005-08-19 | 2007-02-21 | 上海市公安局刑事侦查总队 | Capillary electrophoresis method for detecting medications and poisons in blood and urine at the same time |
| US20080020386A1 (en) * | 2006-03-29 | 2008-01-24 | Medigen Biotechnology Corporation | Methods and apparatus for genotyping |
| CN108535349A (en) * | 2018-04-09 | 2018-09-14 | 天津农学院 | A kind of method of NO3-N and NO2-N in quick detection fruits and vegetables and meat products |
| CN109709198A (en) * | 2018-12-29 | 2019-05-03 | 杭州师范大学 | A kind of on-line preconcentration method of Capillary Electrophoresis |
Non-Patent Citations (2)
| Title |
|---|
| NAN-SOOK HONG ET AL: "Rapid and accurate determination of deoxyribonucleoside monophosphates from DNA using micellar electrokinetic chromatography with a cationic surfactant additive", 《ANAL BIOANAL CHEM》 * |
| 张薇 等: "毛细管电泳中高盐样品在线富集的研究进展", 《分析化学》 * |
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